CN116981283A - Light emitting device, method of manufacturing the same, and display apparatus - Google Patents
Light emitting device, method of manufacturing the same, and display apparatus Download PDFInfo
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- CN116981283A CN116981283A CN202210395518.4A CN202210395518A CN116981283A CN 116981283 A CN116981283 A CN 116981283A CN 202210395518 A CN202210395518 A CN 202210395518A CN 116981283 A CN116981283 A CN 116981283A
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/14—Carrier transporting layers
- H10K50/16—Electron transporting layers
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/14—Carrier transporting layers
- H10K50/16—Electron transporting layers
- H10K50/165—Electron transporting layers comprising dopants
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/18—Carrier blocking layers
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
Abstract
The application discloses a light-emitting device, a preparation method of the light-emitting device and a display device, wherein the light-emitting device comprises an anode, a cathode which is arranged opposite to the anode, a light-emitting layer which is arranged between the anode and the cathode, and an electron transport layer which is arranged between the cathode and the light-emitting layer, wherein the material of the electron transport layer comprises nano metal oxide and nucleating agent, so that the electron-hole transport matching degree is improved, and the carrier injection balance of the light-emitting device is promoted; the preparation method is to mix the nano metal oxide and the nucleating agent in a solution mode to prepare the electron transport layer, so that the non-spontaneous nucleation of the nano metal oxide is promoted to achieve the purpose of grain refinement, the grain boundary number of the electron transport layer is increased, the grain size of the electron transport layer is increased, the resistance of the electron transport layer is effectively increased, the electron migration difficulty is improved, the electron-hole transport balance is promoted, and the comprehensive performance of the light-emitting device is improved.
Description
Technical Field
The application relates to the technical field of photoelectricity, in particular to a light emitting device, a preparation method of the light emitting device and a display device.
Background
The Light Emitting device includes, but is not limited to, an Organic Light-Emitting Diode (OLED) and a quantum dot Light-Emitting Diode (Quantum Dot Light Emitting Diodes, QLED), and is of a "sandwich" structure, i.e., includes an anode, a cathode, and a Light Emitting layer, wherein the anode and the cathode are disposed opposite to each other, and the Light Emitting layer is disposed between the anode and the cathode. The light emitting principle of the light emitting device is: electrons are injected into the light-emitting area from the cathode of the device, holes are injected into the light-emitting area from the anode of the device, the electrons and the holes are combined in the light-emitting area to form excitons, and photons are released from the combined excitons in a radiation transition mode, so that light is emitted.
Taking a QLED as an example, at present, the QLED has a problem of unbalanced carrier injection, that is, the existing QLED generally has a problem that electron injection is greater than hole injection when in operation, so that an electron accumulation phenomenon occurs in a light-emitting layer, and thus the probability of non-light-emitting recombination (such as auger recombination) is increased, and energy is lost, and the problem of performance attenuation of the QLED occurs in the operation process is caused, for example: reduced luminous efficiency, shortened service life, etc.
Therefore, how to improve the problem of imbalance of carrier injection of the light emitting device is of great significance to the application and development of the light emitting device.
Disclosure of Invention
The application provides a light emitting device, a manufacturing method of the light emitting device and a display device, so as to improve the light emitting efficiency and the service life of the light emitting device.
The technical scheme of the application is as follows:
in a first aspect, the present application provides a light emitting device comprising:
an anode;
a cathode disposed opposite the anode;
a light-emitting layer disposed between the anode and the cathode; and
an electron transport layer disposed between the cathode and the light emitting layer;
the material of the electron transport layer comprises a first compound and a second compound, wherein the first compound is nano metal oxide, and the second compound is a nucleating agent.
Further, the first compound is selected fromZnO、TiO 2 、SnO 2 、BaO、Ta 2 O 3 、ZrO 2 At least one of TiLiO, znGaO, znAlO, znMgO, znSnO, znLiO, inSnO, alZnO, znOCl or ZnOF; the first compound has an average particle diameter of 2nm to 15nm.
Further, the nucleating agent is selected from an organic nucleating agent and/or an inorganic nucleating agent;
the organic nucleating agent is at least one of carboxylate compounds, sorbitol compounds, polymer nucleating agents or beta-crystal nucleating agents, wherein the carboxylate compounds are at least one of sodium succinate, sodium glutarate, sodium caproate, sodium 4-methylpentanoate, adipic acid, aluminum adipate, aluminum tert-butylbenzoate, aluminum benzoate, potassium benzoate, lithium benzoate, sodium cinnamate or sodium beta-naphthoate, the sorbitol compounds are at least one of dibenzylidene sorbitol, di (p-methylbenzylidene) sorbitol or di (p-chloro substituted benzylidene) sorbitol, the polymer nucleating agents are at least one of polyvinylcyclohexane, polyethylene pentane or ethylene/acrylic ester copolymer, and the beta-crystal nucleating agents are at least one of beta-polypropylene;
The inorganic nucleating agent is at least one selected from carbon black, calcium oxide, mica, talcum powder or kaolin.
Further, in the electron transport layer, the first compound: the molar ratio of the second compound is 1: (0.1-0.2).
Further, the material of the light-emitting layer is quantum dots, and the quantum dots are at least one selected from single-component quantum dots, core-shell structure quantum dots, inorganic perovskite quantum dots or organic-inorganic hybrid perovskite quantum dots;
when the quantum dot is selected from a single component quantum dot or a core-shell structure quantum dot, the material of the single component quantum dot, the material of the core-shell structure quantum dot, and the material of the shell of the core-shell structure quantum dot are selected from at least one of a group II-VI compound, a group III-V compound, a group IV-VI compound, or a group I-III-VI compound, independently of each other, wherein the group II-VI compound is selected from CdS, cdSe, CdTe, znS, znSe, znTe, znO, hgS, hgSe, hgTe, cdSeS, cdSeTe, cdSTe, znSeS, znSeTe, znSTe, hgSeS, hgSeTe, hgSTe, cdZnS, cdZnSe, cdZnTe, cdHgS, cdHgSe, cdHgTe, hgZnS, hgZnSe, hgZnTe, cdZnSeS, cdZnSeTe, cdZnSTe, cdHgSeS, cdHgSeTe, cdHgSTe, hgZnSeS, hgZnSeTe or HgZnSTe, said III-V compound being selected from at least one of GaN, gaP, gaAs, gaSb, alN, alP, alAs, alSb, inN, inP, inAs, inSb, gaNP, gaNAs, gaNSb, gaPAs, gaPSb, alNP, alNAs, alNSb, alPAs, alPSb, inNP, inNAs, inNSb, inPAs, inPSb, gaAlNP, gaAlNAs, gaAlNSb, gaAlPAs, gaAlPSb, gaInNP, gaInNAs, gaInNSb, gaInPAs, gaInPSb, inAlNP, inAlNAs, inAlNSb, inAlPAs or InAlPSb, said IV-VI compound being selected from at least one of SnS, snSe, snTe, pbS, pbSe, pbTe, snSeS, snSeTe, snSTe, pbSeS, pbSeTe, pbSTe, snPbS, snPbSe, snPbTe, snPbSSe, snPbSeTe or SnPbSTe, said I-III-VI compound being selected from CuInS 2 、CuInSe 2 Or AgInS 2 At least one of them.
Further, the light emitting device further includes a hole function layer disposed between the anode and the light emitting layer;
the hole function layer comprises a hole injection layer and/or a hole transport layer, when the hole function layer comprises a hole transport layer and a hole injection layer which are stacked, the hole transport layer is close to the light emitting layer, and the hole injection layer is close to the anode;
the hole transport layer is made of NiO or WO 3 、MoO 3 CuO, poly (9, 9-dioctylfluorene-CO-N- (4-butylphenyl) diphenylamine), 3-hexyl-substituted polythiophene, poly (9-vinylcarbazole), poly [ bis (4-phenyl) (4-butylphenyl) amine]At least one of poly (N, N '-bis (4-butylphenyl) -N, N' -diphenyl-1, 4-phenylenediamine-CO-9, 9-dioctylfluorene), 4',4 "-tris (carbazol-9-yl) triphenylamine, 4' -bis (9-carbazol) biphenyl, N '-diphenyl-N, N' -bis (3-methylphenyl) -1,1 '-biphenyl-4, 4' -diamine or N, N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine;
the cavity is injected withThe material of the inlet layer is selected from poly (3, 4-ethylenedioxythiophene): at least one of poly (styrenesulfonic acid), copper phthalocyanine, 2,3,5, 6-tetrafluoro-7, 7', 8' -tetracyanodimethyl-p-benzoquinone, 2,3,6,7,10, 11-hexacyano-1, 4,5,8,9, 12-hexaazabenzophenanthrene, transition metal oxide or transition metal chalcogenide, wherein the transition metal oxide is selected from NiO x 、MoO x 、WO x Or CrO (CrO) x At least one of the transition metal chalcogenide compounds is selected from MoS x 、MoSe x 、WS x 、WSe x Or at least one of CuS.
In a second aspect, the present application provides a method for manufacturing a light emitting device, the method comprising the steps of:
providing a laminated structure, applying a mixed solution containing a first compound and a second compound on one side of the laminated structure, and drying to obtain an electron transport layer;
wherein the first compound is nano metal oxide, and the second compound is a nucleating agent;
when the light-emitting device is of a positive structure, the laminated structure is a substrate comprising an anode and a light-emitting layer, and the electron transport layer is formed on one side of the light-emitting layer away from the anode;
when the light emitting device is of an inverted structure, the stacked structure is a substrate including a cathode, and the electron transport layer is formed on one side of the cathode.
Further, the second compound is a solid, and in the mixed liquid, the first compound: the mass ratio of the second compound is 1: (0.02-0.05).
Further, the second compound is a liquid, and the preparation method of the mixed liquid comprises the following steps: providing a solution containing a first compound, and mixing the second compound with the solution containing the first compound to obtain the mixed solution;
Wherein, in the solution containing the first compound, the concentration of the first compound is 30mg/mL to 60mg/mL;
the solution comprising the first compound: the volume ratio of the second compound is 1: (0.01-0.0125).
Further, the step of applying a mixed solution containing a first compound and a second compound on one side of the laminated structure includes the steps of: providing a mixed solution containing a first compound and a second compound, and placing the mixed solution in an alternating current electric field for treatment for a preset time.
Further, the intensity of the alternating current electric field is 100V/m to 500V/m, the frequency of the alternating current electric field is 50Hz to 100Hz, and the effective voltage value of the alternating current electric field is 100V to 200V; the preset time is 1min to 5min.
In a third aspect, the present application provides a display apparatus comprising a light-emitting device according to any one of the first aspects, or a light-emitting device produced by any one of the production methods according to the second aspects.
The application provides a light emitting device, a preparation method of the light emitting device and a display device, which have the following technical effects:
in the light-emitting device, the nucleating agent is added in the electron transport layer, so that the non-spontaneous nucleation of the nano metal oxide can be promoted to increase the number of nuclei, the purpose of refining the crystal grains of the nano metal oxide is achieved, the grain boundary number of the electron transport layer is increased, the grain size of the electron transport layer is increased, the grain boundary potential barrier is increased accordingly, the resistance of the electron transport layer is effectively improved, the electron migration difficulty is increased, the electron mobility of the light-emitting device is reduced, and the electron injection level of the light-emitting device in the embodiment of the application is lower than that of the existing light-emitting device under the same electrifying condition, so that the problem that the electron injection of the existing light-emitting device is greater than that of the hole injection is solved, the electron-hole transport matching degree is improved, the carrier injection balance of the light-emitting device is effectively promoted, and the light-emitting efficiency and the service life of the light-emitting device are improved.
In the preparation method of the light-emitting device, the nano metal oxide and the nucleating agent are mixed in a solution mode to prepare the electron transport layer, so that the number of heterogeneous cores is increased, the non-spontaneous nucleation of the nano metal oxide is promoted to achieve the purpose of grain refinement, the grain boundary number of the electron transport layer is increased, the grain size of the electron transport layer is increased, the grain boundary potential barrier is increased accordingly, the resistance of the electron transport layer is effectively increased, the electron migration difficulty is improved, the electron injection level is reduced, the electron-hole transport balance is promoted, and the light-emitting efficiency and the service life of the light-emitting device are further improved.
The light-emitting device is applied to the display device, and is beneficial to improving the display effect of the display device and prolonging the service life of the display device.
Drawings
The technical solution and other advantageous effects of the present application will be made apparent by the following detailed description of the specific embodiments of the present application with reference to the accompanying drawings.
Fig. 1 is a schematic structural view of a first light emitting device according to an embodiment of the present application.
Fig. 2 is a schematic structural view of a second light emitting device according to an embodiment of the present application.
Fig. 3 is a schematic diagram showing the grain size of the electron transport layer according to the embodiment of the present application under different processing modes.
Fig. 4 is a schematic structural view of a third light emitting device according to an embodiment of the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. It will be apparent that the described embodiments are only some, but not all, embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to fall within the scope of the application.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the present application. The preferred methods and materials described herein are illustrative only and should not be construed as limiting the application.
The following description of the embodiments is not intended to limit the preferred embodiments. In addition, in the description of the present application, the term "comprising" means "including but not limited to". Various embodiments of the application may exist in a range of forms; it should be understood that the description in a range format is merely for convenience and brevity and should not be construed as a rigid limitation on the scope of the application; it is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the ranges, such as 1, 2, 3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
The embodiment of the application provides a light emitting device, as shown in fig. 1, the light emitting device 1 comprises an anode 11, a cathode 12, a light emitting layer 13 and an electron transport layer 14, wherein the anode 11 is opposite to the cathode 12, the light emitting layer 13 is arranged between the anode 11 and the cathode 12, and the electron transport layer 14 is arranged between the cathode 12 and the light emitting layer 13.
The material of the electron transport layer 14 includes a first compound and a second compound, wherein the first compound is nano metal oxide, and the second compound is a nucleating agent.
As used in the present application, the term "nucleating agent" is also known as a nucleating agent, and refers to a compound capable of changing the partial crystallization behavior of nano metal oxide, and the action principle is as follows: the nucleation needed by the nucleation of the nano metal oxide is provided, so that the nano metal oxide is converted from homogeneous nucleation to heterogeneous nucleation to increase the number of nuclei, thereby accelerating the crystallization speed, refining the grain structure and ensuring that the grain size of the nano metal oxide does not change obviously. The nucleation agent is added into the electron transport layer, so that the non-spontaneous nucleation of the nano metal oxide can be promoted to refine crystal grains of the nano metal oxide, and the crystal boundary number of the electron transport layer is increased, thereby improving the crystal grain size of the electron transport layer, increasing the crystal boundary potential barrier, effectively improving the resistance of the electron transport layer, further increasing the electron migration difficulty and reducing the electron mobility of the light-emitting device. Therefore, under the same energizing condition, the electron injection level of the light-emitting device is lower than that of the existing light-emitting device, so that the problem that the electron injection is larger than the hole injection of the existing light-emitting device is solved, the electron-hole transmission matching degree is improved, the carrier injection balance of the light-emitting device is effectively promoted, and the light-emitting efficiency and the service life of the light-emitting device are improved.
As used herein, "grain boundaries" refer to interfaces between grains that belong to the same solid phase but are oriented differently.
As used herein, "grain size" is a measure of the average size of grains in a nano-metal oxide; the more grain boundaries, the larger the grain size.
The first compound may be an undoped nano metal oxide or a doped nano metal oxide. In some embodiments of the application, the first compound is selected from ZnO, tiO 2 、SnO 2 、BaO、Ta 2 O 3 、ZrO 2 At least one of TiLiO, znGaO, znAlO, znMgO, znSnO, znLiO, inSnO, alZnO, znOCl or ZnOF. The average particle diameter of the first compound may be, for example, 2nm to 15nm.
The second compound is selected from an organic nucleating agent and/or an inorganic nucleating agent, the organic nucleating agent is selected from at least one of carboxylate metal salt compounds, sorbitol compounds, polymer nucleating agents or beta crystal form nucleating agents, wherein the carboxylate metal salt compounds are selected from at least one of sodium succinate, sodium glutarate, sodium caproate, sodium 4-methylpentanoate, adipic acid, aluminum adipate, aluminum tert-butylbenzoate, aluminum benzoate, potassium benzoate, lithium benzoate, sodium cinnamate or sodium beta-naphthoate, the sorbitol compounds are selected from at least one of dibenzylidene sorbitol, di (p-methyl benzylidene) sorbitol or di (p-chloro substituted benzylidene) sorbitol, the polymer nucleating agents are selected from at least one of polyvinylcyclohexane, polyvinylpentane or ethylene/acrylate copolymer, and the beta crystal form nucleating agents are selected from beta polypropylene; the inorganic nucleating agent is at least one selected from carbon black, calcium oxide, mica, talcum powder or kaolin.
In at least one embodiment of the present application, the second compound is selected from dibenzylidene sorbitol, which has the advantages of low cost, availability and little environmental hazard, and furthermore, since dibenzylidene sorbitol is a colorless material, dibenzylidene sorbitol does not affect the transparency of the electron transport layer, and thus does not adversely affect the luminous efficiency of the light emitting device.
In order to further improve the overall performance of the light emitting device, in some embodiments of the present application, the first compound in the electron transport layer: the molar ratio of the second compound is 1: (0.1-0.2), which is beneficial to further promoting the non-spontaneous nucleation of the nano metal oxide and simultaneously maximally improving the matching degree between the electron injection level and the hole injection level of the light-emitting device.
In the light emitting device of the embodiment of the present application, materials of the anode 11, the cathode 12, and the light emitting layer 13 may be materials common in the art, for example:
the materials of the anode 11 and the cathode 12 are independently selected from at least one of metal, carbon material or metal oxide, and the metal is selected from at least one of Al, ag, cu, mo, au, ba, ca or Mg; the carbon material is at least one of graphite, carbon nano tube, graphene or carbon fiber; the metal oxide may be a doped or undoped metal oxide, for example, at least one selected from Indium Tin Oxide (ITO), fluorine doped tin oxide (FTO), tin antimony oxide (ATO), aluminum doped zinc oxide (AZO), gallium doped zinc oxide (GZO), indium doped zinc oxide (IZO) or magnesium doped zinc oxide (MZO). Anode 11 or cathode 12 may also be selected from a composite electrode of doped or undoped transparent metal oxide sandwiching a metal, the composite electrode including but not limited to AZO/Ag/AZO, AZO/Al/AZO, ITO/Ag/ITO, ITO/Al/ITO, znO/Ag/ZnO, znO/Al/ZnO, tiO 2 /Ag/TiO 2 、TiO 2 /Al/TiO 2 、ZnS/Ag/ZnS、ZnS/Al/ZnS、TiO 2 /Ag/TiO 2 Or TiO 2 /Al/TiO 2 At least one of them. The thickness of the anode 11 may be, for example, 40nm to 160nm, and the thickness of the cathode 12 may be, for example, 20nm to 120nm.
The material of the light emitting layer 13 is a quantum dot, and the thickness of the light emitting layer 13 may be, for example, 20nm to 100nm. The quantum dots include, but are not limited to, at least one of red, green, or blue quantum dots, and the quantum dots include, but are not limited to, at least one of single component quantum dots, core-shell structure quantum dots, inorganic perovskite quantum dots, or organic-inorganic hybrid perovskite quantum dots. The particle size of the quantum dots may be, for example, 5nm to 10nm.
When the quantum dot is selected from a single component quantum dot or a core-shell structure quantum dot, the material of the single component quantum dot, the material of the core-shell structure quantum dot, and the material of the shell of the core-shell structure quantum dot are selected from at least one of group II-VI compound, group III-V compound, group IV-VI compound, or group I-III-VI compound independently of each other, wherein the group II-VI compound is selected from at least one of CdS, cdSe, cdTe, znS, znSe, znTe, znO, hgS, hgSe, hgTe, cdSeS, cdSeTe, cdSTe, znSeS, znSeTe, znSTe, hgSeS, hgSeTe, hgSTe, cdZnS, cdZnSe, cdZnTe, cdHgS, cdHgSe, cdHgTe, hgZnS, hgZnSe, hgZnTe, cdZnSeS, cdZnSeTe, cdZnSTe, cdHgSeS, cdHgSeTe, cdHgSTe, hgZnSeS, hgZnSeTe or HgZnSTe, the group III-V compound is selected from at least one of GaN, gaP, gaAs, gaSb, alN, alP, alAs, alSb, inN, inP, inAs, inSb, gaNP, gaNAs, gaNSb, gaPAs, gaPSb, alNP, alNAs, alNSb, alPAs, alPSb, inNP, inNAs, inNSb, inPAs, inPSb, gaAlNP, gaAlNAs, gaAlNSb, gaAlPAs, gaAlPSb, gaInNP, gaInNAs, gaInNSb, gaInPAs, gaInPSb, inAlNP, inAlNAs, inAlNSb, inAlPAs or InAlPSb, the group IV-VI compound is selected from at least one of SnS, snSe, snTe, pbS, pbSe, pbTe, snSeS, snSeTe, snSTe, pbSeS, pbSeTe, pbSTe, snPbS, snPbSe, snPbTe, snPbSSe, snPbSeTe or SnPbSTe, and the group I-III-VI compound is selected from CuInS 2 、CuInSe 2 Or AgInS 2 At least one of them.
For the inorganic perovskite quantum dots,the structural general formula of the inorganic perovskite quantum dot is AMX 3 Wherein A is Cs + Ion, M is a divalent metal cation, M includes but is not limited to Pb 2+ 、Sn 2+ 、Cu 2+ 、Ni 2+ 、Cd 2+ 、Cr 2+ 、Mn 2+ 、Co 2+ 、Fe 2+ 、Ge 2+ 、Yb 2+ Or Eu 2+ X is a halogen anion including but not limited to Cl - 、Br - Or I - 。
For the organic-inorganic hybrid perovskite quantum dots, the structural general formula of the organic-inorganic hybrid perovskite quantum dots is BMX 3 Wherein B is an organic amine cation including, but not limited to, CH 3 (CH 2 ) n -2NH 3+ (n.gtoreq.2) or NH 3 (CH 2 ) n NH 3 2+ (n.gtoreq.2), M is a divalent metal cation, M includes but is not limited to Pb 2+ 、Sn 2+ 、Cu 2+ 、Ni 2+ 、Cd 2+ 、Cr 2+ 、Mn 2+ 、Co 2+ 、Fe 2+ 、Ge 2+ 、Yb 2+ Or Eu 2+ X is a halogen anion including but not limited to Cl - 、Br - Or I - 。
It is understood that when the material of the light emitting layer includes quantum dots, the material of the light emitting layer further includes a ligand attached to the surface of the quantum dots, the ligand includes, but is not limited to, at least one of amine ligands, carboxylic acid ligands, thiol ligands, (oxy) phosphine ligands, phospholipids, soft phospholipids, or polyvinylpyridines, the amine ligands are selected from at least one of oleylamine, n-butylamine, n-octylamine, octaamine, or 1, 2-ethylenediamine, the carboxylic acid ligands are selected from at least one of oleic acid, acetic acid, butyric acid, valeric acid, caproic acid, arachidic acid, dodecanoic acid, undecylenic acid, tetradecanoic acid, or stearic acid, the thiol ligands are selected from at least one of ethanethiol, propanethiol, mercaptoethanol, benzenethiol, octanethiol, dodecyl mercaptan, or octadecyl thiol, and the (oxy) phosphine ligands are selected from at least one of trioctylphosphine or trioctylphosphine oxide.
In order to obtain better photoelectric performance and lifetime, in some embodiments of the present application, as shown in fig. 2, the light emitting device 1 further includes a hole function layer 15, and the hole function layer 15 is disposed between the anode 11 and the light emitting layer 13. The hole function layer 15 includes a hole injection layer and/or a hole transport layer, and when the hole function layer includes a hole transport layer and a hole injection layer which are stacked, the hole transport layer is close to the light emitting layer, and the hole injection layer is close to the anode. The thickness of the hole function layer 15 may be, for example, 20nm to 200nm.
The material of the hole transport layer includes, but is not limited to, poly (9, 9-dioctylfluorene-CO-N- (4-butylphenyl) diphenylamine) (abbreviated as TFB, CAS number 220797-16-0), 3-hexyl-substituted polythiophene (CAS number 104934-50-1), poly (9-vinylcarbazole) (abbreviated as PVK, CAS number 25067-59-8), poly [ bis (4-phenyl) (4-butylphenyl) amine]At least one of (abbreviated as Poly-TPD, CAS number 472960-35-3), poly (N, N '-bis (4-butylphenyl) -N, N' -diphenyl-1, 4-phenylenediamine-CO-9, 9-dioctylfluorene) (abbreviated as PFB, CAS number 223569-28-6), 4 '-tris (carbazol-9-yl) triphenylamine (abbreviated as TCTA, CAS number 139092-78-7), 4' -bis (9-carbazole) biphenyl (abbreviated as CBP, CAS number 58328-31-7), N '-diphenyl-N, N' -bis (3-methylphenyl) -1,1 '-biphenyl-4, 4' -diamine (abbreviated as TPD, CAS number 65181-78-4) or N, N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine (abbreviated as NPB, CAS number 123847-85-8); in addition, the material of the hole transport layer can be selected from inorganic materials with hole transport capability, including but not limited to NiO, WO 3 、MoO 3 Or CuO. The thickness of the hole transport layer may be, for example, 20nm to 100nm.
The material of the hole injection layer includes, but is not limited to, poly (3, 4-ethylenedioxythiophene): one or more of poly (styrenesulfonic acid) (CAS number 155090-83-8), copper phthalocyanine (abbreviated as CuPc, CAS number 147-14-8), 2,3,5, 6-tetrafluoro-7, 7', 8' -tetracyanodimethyl-p-benzoquinone (abbreviated as F4-TCNQ, CAS number 29261-33-4), 2,3,6,7,10, 11-hexacyano-1, 4,5,8,9, 12-hexaazabenzophenanthrene (abbreviated as HATCN, CAS number 105598-27-4), transition metal oxide or transition metal chalcogenide, wherein the transition metal oxide may be NiO x 、MoO x 、WO x Or CrO (CrO) x The metal chalcogenide may be MoS x 、MoSe x 、WS x 、WSe x Or at least one of CuS. The thickness of the hole transport layer may be, for example, 20nm to 100nm.
The light emitting device may further include other layer structures, for example, the light emitting device may further include an electron injection layer disposed between the electron transport layer and the cathode, the material of the electron injection layer including, but not limited to, at least one of an alkali metal halide including, but not limited to, liF, an alkali metal organic complex including, but not limited to, lithium 8-hydroxyquinoline, or an organic phosphine compound including, but not limited to, at least one of an organic phosphorus oxide, an organic thiophosphine compound, or an organic selenophosphine compound.
The embodiment of the application also provides a preparation method of the light-emitting device, which comprises the following steps:
providing a laminated structure, applying a mixed solution containing a first compound and a second compound on one side of the laminated structure, and drying to obtain an electron transport layer; wherein the first compound is nano metal oxide, and the second compound is nucleating agent; when the light-emitting device is of a positive structure, the laminated structure is a substrate comprising an anode and a light-emitting layer, and the electron transport layer is formed on one side of the light-emitting layer away from the anode; when the light emitting device is of an inverted structure, the stacked structure is a substrate including a cathode, and the electron transport layer is formed on one side of the cathode.
It should be noted that, the selection types of the nano metal oxide and the nucleating agent refer to the foregoing description, and are not repeated here; the application mode of the mixed liquid comprises at least one of spin coating, ink-jet printing, knife coating, dip-coating, dipping, spraying, roll coating or casting. The nano metal oxide and the nucleating agent are mixed in a solution mode to increase the number of heterogeneous cores, promote the non-spontaneous nucleation of the nano metal oxide to achieve the purpose of grain refinement, increase the grain boundary number of the electron transport layer, thereby improving the grain size of the electron transport layer, increasing the grain boundary barrier along with the grain boundary barrier, effectively increasing the resistance of the electron transport layer, improving the electron migration difficulty, reducing the electron injection level, promoting the electron-hole transport balance, and further improving the luminous efficiency and the service life of the light-emitting device.
Further, as used herein, "drying process" includes all processes that enable the wet film to be converted to a dry film with higher energy, including but not limited to heat treatment and standing for natural drying, wherein "heat treatment" may be constant temperature heat treatment or non-constant temperature heat treatment (e.g., temperature gradient change), and in at least one embodiment of the present application "drying process" refers to constant temperature heat treatment at 100 ℃ to 200 ℃ for 15min to 30min.
In some embodiments of the application, the second compound is a solid, and in the mixed liquor, the first compound: the mass ratio of the second compound is 1: (0.02-0.05), the content of the second compound in the mixed solution is too high or too low, so that the comprehensive performance improvement effect of the light-emitting device is limited, and if the content of the second compound is too low, the promotion effect on the non-spontaneous nucleation of the nano metal oxide is limited, so that the improvement degree of the resistance of the electron transport layer is limited; if the content of the second compound is too high, the degree of improvement in the degree of matching between the electron injection level and the hole injection level of the light emitting device is limited. The solvent of the mixed solution is at least one selected from ethanol, ethylene glycol methyl ether and glacial acetic acid.
In other embodiments of the present application, the second compound is a liquid and the method of preparing the mixture comprises the steps of: providing a solution containing a first compound, and mixing a second compound with the solution containing the first compound to prepare a mixed solution; wherein the concentration of the first compound in the solution comprising the first compound is from 30mg/mL to 60mg/mL, the solution comprising the first compound: the volume ratio of the second compound is 1: (0.01 to 0.0125), as described above, the addition amount of the second compound for preparing the mixed solution is too large or too small to have a limited effect on the overall performance improvement of the light emitting device. The solvent in the solution containing the first compound is at least one selected from ethanol, ethylene glycol methyl ether, and glacial acetic acid.
In order to further promote electron-hole transport equilibrium of the light emitting device, the application of a mixed solution containing a first compound and a second compound on one side of the laminated structure, comprising the steps of: providing a mixed solution containing a first compound and a second compound, and placing the mixed solution in an alternating current electric field for processing for a preset time. As shown in fig. 3, a is the grain size of the electron transport layer to which the nucleating agent is not added, B is the grain size of the electron transport layer to which the nucleating agent is added, C is the grain size of the electron transport layer to which the nucleating agent is added after the alternating electric field treatment, wherein cracks represent grain boundaries, the more the cracks are, the larger the grain boundaries are correspondingly, the grain size of C is the largest, and the grain size of a is the smallest, which means: the mixed liquid is treated by adopting an alternating current electric field, so that grain refinement can be further promoted, the resistance of an electron transport layer is further improved, and the matching degree of the electron injection level and the hole injection level of the light-emitting device is further improved.
In some embodiments of the present application, the intensity of the alternating current electric field is 100V/m to 500V/m, the frequency of the alternating current electric field is 50Hz to 100Hz, the effective voltage value of the alternating current electric field is 100V to 200V, and the preset time is 1min to 5min.
In some embodiments of the present application, when the light emitting device is in a front-mounted structure, the manufacturing method further includes the steps of: and preparing and forming a cathode on one side of the electron transport layer far away from the light emitting layer.
It is understood that when the light emitting device is in a front structure, the stacked structure may be, for example, a substrate including an anode, a hole function layer, and a light emitting layer, the anode is disposed opposite to the light emitting layer, the hole function layer is disposed between the anode and the light emitting layer, and the electron transport layer is formed on a side of the light emitting layer away from the hole function layer.
In one embodiment of the present application, when the light emitting device is in a front structure, the manufacturing method includes the steps of:
s1, providing a substrate, and preparing and forming an anode on one side of the substrate;
s2, preparing and forming a hole function layer on one side of the anode far away from the substrate;
s3, preparing a luminescent layer on one side of the hole functional layer far away from the anode;
s4, applying a mixed solution containing a first compound and a second compound on one side of the light-emitting layer far away from the hole function layer, and drying to obtain an electron transport layer;
S5, preparing and forming a cathode on one side of the electron transport layer far away from the light emitting layer.
In another embodiment of the present application, when the light emitting device is of a front structure, the difference is only that, compared to the aforementioned method for manufacturing the light emitting device having the front structure: and replacing the step S4 with providing a mixed solution containing the first compound and the second compound, placing the mixed solution in an alternating electric field for treatment for a preset time to obtain a reaction solution, then applying the reaction solution on the side of the light-emitting layer far away from the hole functional layer, and drying to obtain the electron transport layer.
In other embodiments of the present application, when the light emitting device is of an inverted structure, the manufacturing method further includes the steps of:
preparing a light-emitting layer on one side of the electron transport layer far away from the cathode; and
an anode is formed on the side of the light-emitting layer away from the electron transport layer.
Further, when the light emitting device is in an inverted structure, the anode is formed on the side of the light emitting layer far away from the electron transport layer, and the method comprises the following steps:
preparing a hole function layer on one side of the light-emitting layer far away from the electron transport layer; and
an anode is formed on the side of the hole function layer away from the light-emitting layer.
In one embodiment of the present application, when the light emitting device is of an inverted structure, the manufacturing method includes the steps of:
s1', providing a substrate, and preparing and forming a cathode on one side of the substrate;
s2', applying a mixed solution containing a first compound and a second compound on one side of the cathode away from the substrate, and drying to obtain an electron transport layer;
s3', preparing and forming a light-emitting layer on one side of the electron transport layer far away from the cathode;
s4', preparing and forming a hole functional layer on one side of the light-emitting layer far away from the electron transport layer;
s5', preparing and forming an anode on one side of the hole functional layer far away from the light-emitting layer.
In another embodiment of the present application, when the light emitting device is of an inverted structure, the difference is only that, compared to the aforementioned manufacturing method of the light emitting device having an inverted structure: step S4 is replaced by "providing a mixed solution containing the first compound and the second compound, placing the mixed solution in an alternating electric field for a preset time to obtain a reaction solution, then applying the reaction solution on the side of the cathode away from the substrate, and drying to obtain the electron transport layer.
Besides the electron transport layer, the preparation method of each other film layer in the light-emitting device comprises a solution method and a deposition method, wherein the solution method comprises, but is not limited to, spin coating, ink-jet printing, knife coating, dip-coating, dipping, spraying, roll coating or casting; the deposition method includes a chemical method including, but not limited to, a chemical vapor deposition method, a continuous ion layer adsorption and reaction method, an anodic oxidation method, an electrolytic deposition method, or a coprecipitation method, and a physical method including, but not limited to, a thermal evaporation plating method, an electron beam evaporation plating method, a magnetron sputtering method, a multi-arc ion plating method, a physical vapor deposition method, an atomic layer deposition method, or a pulsed laser deposition method. When the film layer is prepared by a solution method, a drying treatment process is added to convert the wet film into a dry film.
It will be appreciated that the method of manufacturing a light emitting device may also include other steps, such as: after each layer of the light emitting device is completed, the light emitting device is subjected to a packaging process.
The embodiment of the application also provides a display device which comprises the light-emitting device or the light-emitting device manufactured by the manufacturing method of any one of the light-emitting devices. The display device may be any electronic product with a display function, including but not limited to a smart phone, a tablet computer, a notebook computer, a digital camera, a digital video camera, a smart wearable device, a smart weighing electronic scale, a vehicle-mounted display, a television set or an electronic book reader, wherein the smart wearable device may be, for example, a smart bracelet, a smart watch, a Virtual Reality (VR) helmet, etc.
The technical solutions and effects of the present application will be described in detail by way of specific examples, comparative examples and experimental examples, which are only some examples of the present application, and are not intended to limit the present application in any way.
Example 1
The present embodiment provides a light emitting device and a method for manufacturing the same, wherein the light emitting device is a quantum dot light emitting diode with a front-mounted structure, and as shown in fig. 4, the light emitting device 1 includes a substrate 10, an anode 11, a hole injection layer 151, a hole transport layer 152, a light emitting layer 13, an electron transport layer 14, and a cathode 12, which are sequentially disposed in a bottom-to-top direction.
The materials and thicknesses of the respective layers in the light emitting device 1 are as follows:
the material of the substrate 10 is glass, and the thickness of the substrate 10 is 1mm;
the anode 11 is made of ITO, and the thickness of the anode 11 is 25nm;
the cathode 12 is made of Ag, and the thickness of the cathode 12 is 35nm;
the luminescent layer 13 is made of ZnCdS/ZnS quantum dots (the surface of which is connected with octathiol ligand), and the thickness of the luminescent layer 13 is 60nm;
the material of the electron transport layer 14 is composed of a first compound and a second compound, the first compound being nano ZnO (particle size of 12 nm); the second compound is dibenzylidene sorbitol, the first compound: the molar ratio of the second compound is 1:0.15, the thickness of the electron transport layer 14 is 60nm;
the hole injection layer 151 is made of PEDOT PSS with the thickness of 50nm;
the hole transport layer 152 is of TFB and has a thickness of 50nm.
The preparation method of the light-emitting device in the embodiment comprises the following steps:
s1.1, providing a substrate, sputtering ITO on one side of the substrate to obtain an ITO layer, dipping a small amount of soapy water on the surface of the ITO layer by using a cotton swab to wipe the surface of the ITO layer so as to remove impurities visible to the naked eyes on the surface, sequentially ultrasonically cleaning the substrate comprising the ITO by using deionized water, acetone for 15min, ethanol for 15min and isopropanol for 15min, and performing ultraviolet-ozone surface treatment for 15min after drying to obtain the substrate comprising an anode;
S1.2, spin-coating PEDOT on one side of the anode far away from the substrate in the step S1.1 under the atmospheric environment of normal temperature and normal pressure: performing constant temperature heat treatment on the PSS aqueous solution at 150 ℃ for 20min to obtain a hole injection layer;
s1.3, spin-coating TFB-chlorobenzene solution on one side of the hole injection layer far away from the anode in the step S1.2 under the nitrogen environment of normal temperature and normal pressure, and then placing the film at a constant temperature of 150 ℃ for heat treatment for 20min to obtain a hole transport layer;
s1.4, spin-coating a ZnCdS/ZnS quantum dot-n-octane solution with the concentration of 20mg/mL on one side of the hole transport layer far away from the hole injection layer in the step S1.3 under the nitrogen environment of normal temperature and normal pressure, and then placing the solution in a constant temperature heat treatment for 10min at 100 ℃ to obtain a luminescent layer;
s1.5, providing a 45mg/mL nano ZnO (particle size of 12 nm) -ethanol solution, dissolving 1mL dibenzylidene sorbitol in 99mL nano ZnO (particle size of 12 nm) -ethanol solution to prepare a mixed solution, spin-coating the mixed solution on one side of a luminescent layer far away from a hole transport layer in the step S1.4 in a nitrogen environment at normal temperature and normal pressure, and then placing the mixed solution at a constant temperature of 150 ℃ for heat treatment for 20min to obtain an electron transport layer;
s1.6 at an air pressure of 4X 10 -6 And (3) evaporating Ag on one side of the electron transport layer far away from the light-emitting layer in the step S1.5 in a vacuum environment of mbar to obtain a cathode, and then packaging by ultraviolet curing glue to obtain the light-emitting device.
Example 2
The present embodiment provides a light emitting device and a method for manufacturing the same, which differ from the light emitting device of embodiment 1 only in that: a first compound: the molar ratio of the second compound is 1:0.1.
the manufacturing method of the light emitting device in this embodiment differs from that of embodiment 1 only in that: the step S1.5 was replaced with "providing a nano ZnO (particle size of 12 nm) -ethanol solution having a concentration of 60 mg/mL", 1mL of dibenzylidene sorbitol was dissolved in 99mL of the nano ZnO (particle size of 12 nm) -ethanol solution to prepare a mixed solution, the mixed solution was spin-coated on the side of the light-emitting layer of the step S1.4 away from the hole transport layer under a nitrogen atmosphere at normal temperature and pressure, and then placed at a constant temperature of 150℃for 20 minutes to obtain an electron transport layer.
Example 3
The present embodiment provides a light emitting device and a method for manufacturing the same, which differ from the light emitting device of embodiment 1 only in that: a first compound: the molar ratio of the second compound is 1:0.2.
the manufacturing method of the light emitting device in this embodiment differs from that of embodiment 1 only in that: the step S1.5 was replaced with "providing 30mg/mL of nano ZnO (particle size 12 nm) -ethanol solution, 1mL of dibenzylidene sorbitol was dissolved in 99mL of nano ZnO (particle size 12 nm) -ethanol solution to prepare a mixed solution, the mixed solution was spin-coated on the side of the light-emitting layer of the step S1.4 away from the hole transport layer under nitrogen atmosphere at normal temperature and pressure, and then placed at a constant temperature of 150℃for 20min to obtain an electron transport layer.
Example 4
The present embodiment provides a light emitting device and a method for manufacturing the same, which differ from the light emitting device of embodiment 1 only in that: a first compound: the molar ratio of the second compound is 1:0.3.
the manufacturing method of the light emitting device in this embodiment differs from that of embodiment 1 only in that: the step S1.5 was replaced with "providing a nano ZnO (particle size of 12 nm) -ethanol solution having a concentration of 15 mg/mL", 1mL of dibenzylidene sorbitol was dissolved in 99mL of the nano ZnO (particle size of 12 nm) -ethanol solution to prepare a mixed solution, the mixed solution was spin-coated on the side of the light-emitting layer of the step S1.4 away from the hole transport layer under a nitrogen atmosphere at normal temperature and pressure, and then placed at a constant temperature of 150℃for 20 minutes to obtain an electron transport layer.
Example 5
The present embodiment provides a light emitting device and a method for manufacturing the same, which differ from the light emitting device of embodiment 1 only in that: a first compound: the molar ratio of the second compound is 1:0.05.
the manufacturing method of the light emitting device in this embodiment differs from that of embodiment 1 only in that: the step S1.5 was replaced with "providing a nano ZnO (particle size of 12 nm) -ethanol solution having a concentration of 120 mg/mL", 1mL of dibenzylidene sorbitol was dissolved in 99mL of the nano ZnO (particle size of 12 nm) -ethanol solution to prepare a mixed solution, the mixed solution was spin-coated on the side of the light-emitting layer of the step S1.4 away from the hole transport layer under a nitrogen atmosphere at normal temperature and pressure, and then placed at a constant temperature of 150℃for 20 minutes to obtain an electron transport layer.
Example 6
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 1, the method for manufacturing a light emitting device in this embodiment is only different in that: replacing the step S1.5 with 'providing a nano ZnO (particle size of 12 nm) -ethanol solution with concentration of 45 mg/mL', dissolving 1mL of dibenzylidene sorbitol in 99mL of the nano ZnO (particle size of 12 nm) -ethanol solution to prepare a mixed solution, and placing the mixed solution under a rectangular alternating current electric field with frequency of 50Hz and voltage of minus 200V to plus 200V for reaction for 1min to obtain a reaction solution; and then spin-coating the reaction liquid on one side of the luminescent layer far away from the hole transport layer in the step S1.4 under the nitrogen environment of normal temperature and normal pressure, and then placing the reaction liquid at a constant temperature of 150 ℃ for heat treatment for 20min to obtain the electron transport layer.
Example 7
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 6, the method for manufacturing a light emitting device in this embodiment is only different in that: the reaction time of the mixed solution under the alternating current field is replaced by '1 min' to '2 min'.
Example 8
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 6, the method for manufacturing a light emitting device in this embodiment is only different in that: the reaction time of the mixed solution under the alternating current field is replaced by '1 min' to '3 min'.
Example 9
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 6, the method for manufacturing a light emitting device in this embodiment is only different in that: the reaction time of the mixed solution under the alternating current field is replaced by '1 min' to '4 min'.
Example 10
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 6, the method for manufacturing a light emitting device in this embodiment is only different in that: the reaction time of the mixed solution under the alternating current field is replaced by '1 min' to '5 min'.
Example 11
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 6, the method for manufacturing a light emitting device in this embodiment is only different in that: the reaction time of the mixed solution under the alternating current field is replaced by '1 min' to '6 min'.
Example 12
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 6, the method for manufacturing a light emitting device in this embodiment is only different in that: the reaction time of the mixed solution under the alternating current field is replaced by '1 min' to '7 min'.
Example 13
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 6, the method for manufacturing a light emitting device in this embodiment is only different in that: the reaction time of the mixed solution under the alternating current field is replaced by '1 min' to '8 min'.
Example 14
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 1, the method for manufacturing a light emitting device in this embodiment is only different in that: the step S1.5 was replaced with "providing a nano ZnO (particle size of 12 nm) -ethanol solution having a concentration of 45 mg/mL", 315mg of sodium succinate was dissolved in 100mL of the nano ZnO (particle size of 12 nm) -ethanol solution to prepare a mixed solution, and then the mixed solution was spin-coated on the side of the light emitting layer of the step S1.4 away from the hole transporting layer under a nitrogen atmosphere at normal temperature and pressure, and then subjected to constant temperature heat treatment at 150℃for 20 minutes to obtain an electron transporting layer ".
Example 15
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 1, the method for manufacturing a light emitting device in this embodiment is only different in that: replacing the step S1.5 with 'providing a nano ZnO (particle size of 12 nm) -ethanol solution with concentration of 45 mg/mL', dissolving 315mg of sodium succinate in 100mL of the nano ZnO (particle size of 12 nm) -ethanol solution to prepare a mixed solution, and placing the mixed solution under a rectangular alternating current electric field with frequency of 50Hz and voltage of minus 200V to plus 200V for reaction for 5min to obtain a reaction solution; and then spin-coating the reaction liquid on one side of the luminescent layer far away from the hole transport layer in the step S1.4 under the nitrogen environment of normal temperature and normal pressure, and then placing the reaction liquid at a constant temperature of 150 ℃ for heat treatment for 20min to obtain the electron transport layer.
Example 16
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 1, the method for manufacturing a light emitting device in this embodiment is only different in that: the step S1.5 was replaced with "providing a nano ZnO (particle size of 12 nm) -ethanol solution having a concentration of 45 mg/mL", 1mL of beta-type polypropylene was dissolved in 99mL of the nano ZnO (particle size of 12 nm) -ethanol solution to prepare a mixed solution, and then the mixed solution was spin-coated on the side of the light-emitting layer of the step S1.4 remote from the hole transport layer under a nitrogen atmosphere at normal temperature and pressure, and then subjected to constant temperature heat treatment at 150℃for 20 minutes to obtain an electron transport layer ".
Example 17
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 1, the method for manufacturing a light emitting device in this embodiment is only different in that: replacing the step S1.5 with 'providing a nano ZnO (particle size of 12 nm) -ethanol solution with concentration of 45 mg/mL', dissolving 1mL of beta-polypropylene in 99mL of the nano ZnO (particle size of 12 nm) -ethanol solution to prepare a mixed solution, and placing the mixed solution under a rectangular alternating current electric field with frequency of 50Hz and voltage of minus 200V to plus 200V for reaction for 5min to obtain a reaction solution; and then spin-coating the reaction liquid on one side of the luminescent layer far away from the hole transport layer in the step S1.4 under the nitrogen environment of normal temperature and normal pressure, and then placing the reaction liquid at a constant temperature of 150 ℃ for heat treatment for 20min to obtain the electron transport layer.
Example 18
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 1, the method for manufacturing a light emitting device in this embodiment is only different in that: step S1.5 was replaced with "providing a nano ZnO (particle size of 12 nm) -ethanol solution having a concentration of 45 mg/mL", 1575mg of mica was dissolved in 100mL of the nano ZnO (particle size of 12 nm) -ethanol solution to prepare a mixed solution, and then the mixed solution was spin-coated on the side of the light-emitting layer of step S1.4 away from the hole transport layer under a nitrogen atmosphere at normal temperature and pressure, and then subjected to constant temperature heat treatment at 150℃for 20 minutes to obtain an electron transport layer ".
Example 19
The present embodiment provides a method for manufacturing a light emitting device and a light emitting device manufactured by the same, and compared with the method for manufacturing a light emitting device in embodiment 1, the method for manufacturing a light emitting device in this embodiment is only different in that: replacing the step S1.5 with 'providing a nano ZnO (particle size of 12 nm) -ethanol solution with concentration of 45 mg/mL', dissolving 1575mg of mica in 100mL of the nano ZnO (particle size of 12 nm) -ethanol solution to prepare a mixed solution, and placing the mixed solution under a rectangular alternating current electric field with frequency of 50Hz and voltage of minus 200V to plus 200V for reaction for 5min to obtain a reaction solution; and then spin-coating the reaction liquid on one side of the luminescent layer far away from the hole transport layer in the step S1.4 under the nitrogen environment of normal temperature and normal pressure, and then placing the reaction liquid at a constant temperature of 150 ℃ for heat treatment for 20min to obtain the electron transport layer.
Comparative example
The present embodiment provides a light emitting device and a method of manufacturing the same, which differ from the light emitting device of embodiment 1 only in that: the electron transport layer is made of nano ZnO with the particle size of 12 nm.
Compared with the preparation method of example 1, the preparation method of this example only differs in that: and replacing the step S1.5 with 'under the nitrogen environment at normal temperature and normal pressure', spin-coating a nano ZnO (particle size of 12 nm) -ethanol solution with concentration of 45mg/mL on the side of the luminescent layer far away from the hole transport layer in the step S1.4, and then placing the nano ZnO into a constant temperature heat treatment for 20min at 150 ℃ to obtain the electron transport layer.
Experimental example
The performance of the light emitting devices of examples 1 to 19 and comparative examples was examined, parameters such as voltage, current, luminance, light emission spectrum, etc., of each light emitting device were obtained by detection using a Friedel-crafts FPD optical property measuring apparatus (efficiency test system constructed by LabView control QE-PRO spectrometer, keithley 2400 and Keithley 6485), then key parameters such as external quantum efficiency (External Quantum Efficiency, EQE), power efficiency, etc., were calculated, and the service lives of the above light emitting devices were tested using a life test apparatus. The external quantum efficiency test method is an integrating sphere test method; the life test adopts a constant current method, under the drive of a constant current (2 mA current), a silicon optical system is adopted to test the brightness change of each light-emitting device, the time (T95, h) required for the brightness to decay from 100% to 95% is recorded, and the time (LT95@1000nit, h) required for the brightness of each light-emitting device to decay from 100% to 95% under the brightness of 1000nit is calculated.
The maximum luminous efficiency (ce@max, cd/a), luminous efficiency at 1000nit luminance (ce@1knit, cd/a) and performance test data of lt95@1000nit of each light emitting device are shown in table 1 below:
table 1 list of performance test data of light emitting devices of examples 1 to 19 and comparative examples
As can be seen from table 1, the light emitting devices of examples 1 to 19 are all significantly superior in overall performance to the light emitting device of the comparative example, taking example 10 as an example, ce@max of the light emitting device of example 10 is 2.0 times that of the comparative example, ce@1knit of the light emitting device of example 10 is 2.4 times that of the comparative example, and lt95@1000nit of the light emitting device of example 10 is 11.6 times that of the comparative example, it is fully explained that: the electron transport layer is prepared by adopting the electron transport material containing the nucleating agent and the nano metal oxide, so that the grain size of the electron transport layer can be increased, the resistance of the electron transport layer is increased, excessive electrons are reduced to be accumulated in the light-emitting layer, the matching degree between the electron injection level and the hole injection level is improved, the carrier balance of the light-emitting device is promoted, and the light-emitting efficiency and the service life of the light-emitting device are further improved.
As can be seen from the performance test data of examples 1 to 5, the light emitting devices of examples 1 to 3 all have better overall performance than the light emitting devices of examples 4 and 5, and therefore, the nano metal oxide in the electron transport layer is preferable: the molar ratio of the nucleating agent is 1: (0.1 to 0.2), the effect of improving the overall performance of the light-emitting device is limited by either too high or too low a content of the nucleating agent, and if the content of the nucleating agent is too low (for example, example 5), the effect of promoting the non-spontaneous nucleation of the nano metal oxide is limited, so that the degree of improvement of the resistance of the electron transport layer is limited; if the content of the nucleating agent is too high (for example, example 4), the degree of improvement in the degree of matching between the electron injection level and the hole injection level of the light emitting device is limited.
As can be seen from the performance test data of examples 1 and 6 to 13, examples 14 and 15, examples 16 and 17, and examples 18 and 19, the overall performance of the light emitting device in examples 6 to 13 is better than that of example 1, and the overall performance of the light emitting device in example 10 is the best, and it is fully explained that: compared with an electron transport layer prepared from mixed liquid which is not treated by an alternating current electric field, the electron transport layer prepared from the mixed liquid which is treated by the alternating current electric field has larger grain size, thereby being more beneficial to improving the comprehensive performance of the light-emitting device, in particular to improving the light-emitting efficiency and the service life of the light-emitting device under low brightness (1000 nit); as can be seen from examples 6 to 13, under the specific ac electric field conditions, the ac electric field treatment time is preferably 1min to 5min, and the effect of 5min is better, the overall performance improvement effect of the light emitting device is limited due to the longer or shorter ac electric field treatment time, and the increase degree of the grain size is limited due to the shorter ac electric field treatment time (for example, example 6), so that the resistance improvement degree of the electron transport layer is limited; if the ac electric field treatment time is long (for example, examples 11 to 13), dislocation may occur to some extent due to the excessively large grain size, and crystal defects may be increased.
As is clear from the performance test data of examples 10, 14 to 19 and comparative example, the mixed liquid for preparing the electron transport layer treated with the ac electric field can achieve the purpose of optimizing the grain size and improving the overall performance of the light emitting device, no matter what nucleating agent is added, dibenzylidene sorbitol is preferable as the nucleating agent because: dibenzylidene sorbitol has the advantages of low cost, easy availability and little environmental hazard, and because the dibenzylidene sorbitol is a colorless material, the transparency of the electron transport layer is not affected, and thus the luminous efficiency of the light-emitting device is not negatively affected.
The light emitting device, the method for manufacturing the light emitting device and the display device provided by the embodiment of the application are described in detail. The principles and embodiments of the present application have been described herein with reference to specific examples, the description of which is only for aiding in the understanding of the technical solution of the present application and its core ideas; those of ordinary skill in the art will appreciate that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the scope of the corresponding technical solutions of the embodiments of the present application.
Claims (12)
1. A light emitting device, the light emitting device comprising:
an anode;
a cathode disposed opposite the anode;
a light-emitting layer disposed between the anode and the cathode; and
an electron transport layer disposed between the cathode and the light emitting layer;
the material of the electron transport layer comprises a first compound and a second compound, wherein the first compound is nano metal oxide, and the second compound is a nucleating agent.
2. The light-emitting device according to claim 1, wherein the first compound is selected from ZnO, tiO 2 、SnO 2 、BaO、Ta 2 O 3 、ZrO 2 At least one of TiLiO, znGaO, znAlO, znMgO, znSnO, znLiO, inSnO, alZnO, znOCl or ZnOF; the first compound has an average particle diameter of 2nm to 15nm.
3. The light emitting device of claim 1, wherein the nucleating agent is selected from an organic nucleating agent and/or an inorganic nucleating agent;
the organic nucleating agent is at least one of carboxylate compounds, sorbitol compounds, polymer nucleating agents or beta-crystal nucleating agents, wherein the carboxylate compounds are at least one of sodium succinate, sodium glutarate, sodium caproate, sodium 4-methylpentanoate, adipic acid, aluminum adipate, aluminum tert-butylbenzoate, aluminum benzoate, potassium benzoate, lithium benzoate, sodium cinnamate or sodium beta-naphthoate, the sorbitol compounds are at least one of dibenzylidene sorbitol, di (p-methylbenzylidene) sorbitol or di (p-chloro substituted benzylidene) sorbitol, the polymer nucleating agents are at least one of polyvinylcyclohexane, polyethylene pentane or ethylene/acrylic ester copolymer, and the beta-crystal nucleating agents are at least one of beta-polypropylene;
The inorganic nucleating agent is at least one selected from carbon black, calcium oxide, mica, talcum powder or kaolin.
4. The light-emitting device according to claim 1, wherein in the electron-transporting layer, the first compound: the molar ratio of the second compound is 1: (0.1-0.2).
5. The light-emitting device according to claim 1, wherein the material of the light-emitting layer is a quantum dot selected from at least one of single component quantum dots, core-shell structure quantum dots, inorganic perovskite quantum dots, or organic-inorganic hybrid perovskite quantum dots;
when the quantum dot is selected from a single component quantum dot or a core-shell structure quantum dot, the material of the single component quantum dot, the material of the core-shell structure quantum dot, and the material of the shell of the core-shell structure quantum dot are selected from at least one of a group II-VI compound, a group III-V compound, a group IV-VI compound, or a group I-III-VI compound, independently of each other, wherein the group II-VI compound is selected from at least one of CdS, cdSe, cdTe, znS, znSe, znTe, znO, hgS, hgSe, hgTe, cdSeS, cdSeTe, cdSTe, znSeS, znSeTe, znSTe, hgSeS, hgSeTe, hgSTe, cdZnS, cdZnSe, cdZnTe, cdHgS, cdHgSe, cdHgTe, hgZnS, hgZnSe, hgZnTe, cdZnSeS, cdZnSeTe, cdZnSTe, cdHgSeS, cdHgSeTe, cdHgSTe, hgZnSeS, hgZnSeTe or HgZnSTe, and the group III-V compound is selected from GaN, gaP, gaAs, gaSb, alN, alP, alAs, alSb, inN, inP, inAs, inSb, gaNP, gaNAs, gaNSb, gaPAs, gaPSb, alNP, alNAs, alNSb, alPAs, alPSb, inNP, inNAs, inNSb, inPAs, inPSb, gaAlNP, gaAlNAs, gaAlNSb, gaAlPAs, gaAlPSb, gaInNP, gaInNAs, gaInNSb, gaInPAs, gaInPSb, inAlNP, inAlNAs, inAlNSb, inAl At least one of PAs or InAlPSb, the IV-VI compound is selected from at least one of SnS, snSe, snTe, pbS, pbSe, pbTe, snSeS, snSeTe, snSTe, pbSeS, pbSeTe, pbSTe, snPbS, snPbSe, snPbTe, snPbSSe, snPbSeTe or SnPbSTe, and the I-III-VI compound is selected from CuInS 2 、CuInSe 2 Or AgInS 2 At least one of them.
6. The light-emitting device according to any one of claims 1 to 5, further comprising a hole functional layer provided between the anode and the light-emitting layer;
the hole function layer comprises a hole injection layer and/or a hole transport layer, when the hole function layer comprises a hole transport layer and a hole injection layer which are stacked, the hole transport layer is close to the light emitting layer, and the hole injection layer is close to the anode;
the hole transport layer is made of NiO or WO 3 、MoO 3 CuO, poly (9, 9-dioctylfluorene-CO-N- (4-butylphenyl) diphenylamine), 3-hexyl-substituted polythiophene, poly (9-vinylcarbazole), poly [ bis (4-phenyl) (4-butylphenyl) amine]At least one of poly (N, N '-bis (4-butylphenyl) -N, N' -diphenyl-1, 4-phenylenediamine-CO-9, 9-dioctylfluorene), 4',4 "-tris (carbazol-9-yl) triphenylamine, 4' -bis (9-carbazol) biphenyl, N '-diphenyl-N, N' -bis (3-methylphenyl) -1,1 '-biphenyl-4, 4' -diamine or N, N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine;
The hole injection layer is made of poly (3, 4-ethylenedioxythiophene): at least one of poly (styrenesulfonic acid), copper phthalocyanine, 2,3,5, 6-tetrafluoro-7, 7', 8' -tetracyanodimethyl-p-benzoquinone, 2,3,6,7,10, 11-hexacyano-1, 4,5,8,9, 12-hexaazabenzophenanthrene, transition metal oxide or transition metal chalcogenide, wherein the transition metal oxide is selected from NiO x 、MoO x 、WO x Or CrO (CrO) x At least one of the transition metal chalcogenide compounds is selected from MoS x 、MoSe x 、WS x 、WSe x Or at least one of CuS.
7. A method of manufacturing a light emitting device, comprising the steps of:
providing a laminated structure, applying a mixed solution containing a first compound and a second compound on one side of the laminated structure, and drying to obtain an electron transport layer;
wherein the first compound is nano metal oxide, and the second compound is a nucleating agent;
when the light-emitting device is of a positive structure, the laminated structure is a substrate comprising an anode and a light-emitting layer, and the electron transport layer is formed on one side of the light-emitting layer away from the anode;
when the light emitting device is of an inverted structure, the stacked structure is a substrate including a cathode, and the electron transport layer is formed on one side of the cathode.
8. The production method according to claim 7, wherein the second compound is a solid, and wherein in the mixed liquid, the first compound: the mass ratio of the second compound is 1: (0.02-0.05).
9. The method of claim 7, wherein the second compound is a liquid, and the method of preparing the mixture comprises the steps of: providing a solution containing a first compound, and mixing the second compound with the solution containing the first compound to obtain the mixed solution;
wherein, in the solution containing the first compound, the concentration of the first compound is 30mg/mL to 60mg/mL;
the solution comprising the first compound: the volume ratio of the second compound is 1: (0.01-0.0125).
10. The method of preparing according to claim 7, wherein the applying a mixed solution containing a first compound and a second compound on one side of the laminated structure comprises the steps of: providing a mixed solution containing a first compound and a second compound, and placing the mixed solution in an alternating current electric field for treatment for a preset time.
11. The method according to claim 10, wherein the intensity of the alternating current electric field is 100V/m to 500V/m, the frequency of the alternating current electric field is 50Hz to 100Hz, and the effective voltage value of the alternating current electric field is 100V to 200V; the preset time is 1min to 5min.
12. A display device characterized in that the display device comprises the light-emitting device according to any one of claims 1 to 6, or the light-emitting device produced by the production method according to any one of claims 7 to 11.
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| CN202210395518.4A CN116981283A (en) | 2022-04-14 | 2022-04-14 | Light emitting device, method of manufacturing the same, and display apparatus |
| PCT/CN2022/140025 WO2023197658A1 (en) | 2022-04-14 | 2022-12-19 | Light-emitting device, preparation method for light-emitting device, and display apparatus |
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| CN202210395518.4A CN116981283A (en) | 2022-04-14 | 2022-04-14 | Light emitting device, method of manufacturing the same, and display apparatus |
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| CN111224000A (en) * | 2018-11-26 | 2020-06-02 | Tcl集团股份有限公司 | Quantum dot light-emitting diode and preparation method thereof |
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